Fast and accurate monitoring of monomer concentration during copolymerization reactions is of much interest. It is known that
near-infrared spectroscopy (NIRS) can be used to monitor polymerization reactions. Here, a free radical solution copolymerization
reaction between methyl methacrylate and N,N-dimethylacrylamide is considered. NIR spectra were measured in-line with a transflectance
probe. The spectra of both involved monomers are very similar, making monitoring with NIRS challenging. It is shown that the
NIRS calibration can be set up with only a few (5) off-line measured mixtures. Several validation methods for such a NIRS
calibration model are discussed and tested. NIRS is used to follow conversion of the two monomers in a copolymerization reaction
on-line.

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